Qualitative Detection Limit Research Articles

Optimization and synthesis of a novel sorbent composite based on magnetic chitosan-amine-functionalized bimetallic MOF for the simultaneous dispersive solid-phase microextraction of four aflatoxins in real water, herbal distillate, and food samples.

Aflatoxins (AFs), an important category of pollutants, are formed in many foods and adversely affect human health. Therefore, their determination is critical to ensuring human food health. An efficient dispersive solid-phase microextraction technique was developed as a simple and straightforward sample preparation technique for determination of four aflatoxins using a high-performance liquid chromatography (HPLC) fluorescence detector. A novel efficient, green sorbent for extracting AFs was synthesized based on hydrothermal and chemical strategies. The amounts of three sorbent components were optimized using a mixture design (simplex lattice design), including 14 experiments. The optimal amount of amino-bimetallic Fe/Ni-MIL-53 nanospheres, chitosan, and magnetic Fe3O4 nanoparticles as sorbent components was 0.87, 0.67, and 0.47 g, respectively. Also, various factors affecting the process of AF determination were studied and optimized in two successive experimental designs, including the definitive screening design and the Box-Behnken design. Under optimal conditions, the linear ranges for measuring aflatoxin B1, aflatoxin B2, aflatoxin G1, and aflatoxin G2 were 0.05-82.6, 0.07-86.4, 0.08-85.7, and 0.07-89.5 ng mL-1, respectively. The relative standard deviations under inter-day and intra-day conditions for measuring AFs at three analyte concentrations were determined in triplicate analysis and were in the ranges of 3.7-4.6% and 4.9-6.1% for water sample analysis, respectively. The qualitative detection limits for determining AFs were between 0.01 and 0.05 ng mL-1. The pre-concentration factor of the method for measuring AFs ranged from 739.7 to 802.1. The proposed method was used for determining AFs in several real samples, including herbal distillate, black tea, corn, and real water samples. The relative recovery and standard deviation were 87.8-97.8% and 4.10-6.82%, respectively.

Multivariate versus univariate spectrum analysis of dentine sialophosphoprotein (DSPP) for root resorption prediction: a clinical trial

BackgroundA force applied during orthodontic treatment induces inflammation to root area and lead to root resorption known as orthodontically induced inflammatory root resorption (OIIRR). Dentine sialophosphoprotein (DSPP) is one of the most abundant non-collagenous proteins in dentine that was released into gingival crevicular fluid (GCF) during OIIRR. The aim of this research is to compare DSPP detection using the univariate and multivariate analysis in predicting classification level of root resorption.MethodsThe subjects for this study consisted of 30 patients in 3 group classified as normal, mild, and severe groups of OIIRR. The GCF samples were taken from upper permanent central incisors in the normal and mild group while the upper primary second molars in the severe group. The DSPP qualitative detection limit was determined by analyzing the whole absorption spectrum utilizing multivariate analysis embedded with different preprocessing method. The multivariate analysis represents the multi-wavelength spectrum while univariate analyzes the absorption of a single wavelength.ResultsThe results showed that the multivariate analysis technique using partial least square-discriminate analysis (PLS-DA) with the preprocess method has successfully improved in classification prediction for the normal and mild group at 0.88 percent accuracy. The multivariate using PLS-DA algorithm with Mean Center preprocess method was able to predict normal and mild tooth resorption classes better than the univariate analysis. The classification parameters have improved in term of the specificity, precision and accuracy.ConclusionTherefore, the multivariate analysis helps to predict an early detection of tooth resorption complimenting the sensitivity of the univariate analysis.Trial registration NCT 05077878 (14/10/2021).

Electrochemical studies of lateral flow assay test results for procalcitonin detection

In this study, the lateral flow assay (LFA) has been developed for the detection of bacterial infection (BI) by specific biomarker procalcitonin (PCT), without a need for complicated instrumentations and technical expertise. For the development of the assay, gold nanoparticles (AuNP) and their conjugates with antibodies specific to the model antigen PCT are assessed. Polyclonal antibody (pAb) labelled with gold nanoparticles (AuNP) to obtain the AuNP-pAb complex and the specific monoclonal antibody (mAb) have been dropped at the test zone. This complex is placed over the conjugate line of the LFA strip. In the absence of PCT or the presence of other biomarkers, the test line remained colourless, which revealed the specificity of assay towards PCT among a pool of various analytes. Herein, observations have been made through two different platforms for quantitative and qualitative analysis for the detection of PCT biomarker. The qualitative analysis has been performed on the basis of appearance red color in the test band, while for quantitative analysis, a novel approach has been adopted. Herein, the nitrocellulose membrane (paper strip) is cut out from the LFA strip and used for electrochemical studies under similar solution conditions. Different paper strips presented different cyclic voltammograms (CV) that could be correlated to varying PCT concentrations captured at the test line of the paper strip. The qualitative detection limit for PCT using this LFA was determined to be 2 ng/ml and the quantitative detection limit was 1 ng/ml. The electrochemical response studies of the paper strip by CV technique revealed the sensitivity value of 0.695 mA ng/ml.

A portable 3D-printed biosensing device for rapid detection of genetically modified maize MON810

Portable 3D-printed biosensing devices have high potential as analytical platforms due to their unique characteristics. In this study, an easy-to-use biosensing device was constructed based on an event-specific recombinase polymerase amplification-lateral flow strip (RPA-LFS) method for rapid detection of genetically modified maize, MON810. We first established a rapid method for genomic DNA extraction, which achieved rapid extraction in 5 min and does not require professional equipment. The extracted DNA was then used for event-specific RPA amplification and LFS detection in a self-designed 3D-printed device that realized the detection of genetically modified maize MON810 in less than 25 min. The whole process from raw material processing to detection was rapid and easy to use. The qualitative detection limit of the method established in this study was 0.1 wt%, which meets the requirements of most countries and regions in the world for the detection of genetically modified ingredients. The results indicated that the portable 3D-printed biosensing device was sensitive and reliable with actual samples and has the potential to be applied to the rapid screening of risk factors for food safety.

Genetic Detection of Neospora caninum in the Blood of Dairy Cattle from Boyacá, Colombia

Neospora caninum is a parasite of the phylum Apicomplexa that causes significant economic losses for cattle husbandry worldwide. Despite its relevance, information regarding infection prevalence in endemic areas of Colombia is scarce. Previous studies have reported a high seroprevalence in dairy cattle from Boyacá, which suggests a significant risk factor for active transmission of neosporosis. However, there is no available data concerning the infection stage or the presence of said parasite in the peripheral blood of dairy cattle. In this study, genetic detection of N. caninum was carried out using a nested PCR with an Nc-5 marker on peripheral blood samples from dairy cows in the municipalities of Paipa, Toca, and Tuta. Four positive samples were sequenced through the Sanger method, which were then edited, aligned, and compared to sequences available in the GenBank database. The parasite’s DNA was detected in 23 out of 170 analyzed blood samples. A qualitative detection limit was estimated (~64 parasites per volume of blood sampled). This is the first report of DNA detection of N. caninum through PCR in blood from Colombian dairy cattle. Thereupon, further studies about N. caninum molecular detection and population genetics in cattle peripheral blood could be very useful for the early diagnosis of neosporosis and creating more effective epidemiological surveillance strategies.

Ag nano-assemblies on Si surface via CTAB-assisted galvanic reaction for sensitive and reliable surface-enhanced Raman scattering detection

In this work, we report a quick and controllable method for fabricating Ag nanoparticles (NPs) and nano-assemblies (NAs) on silicon (Si) surface via a galvanic reaction assisted by surfactant hexadecyltrimethylammonium bromide (CTAB). Obtained Si substrates with high density Ag NAs serve as surface-enhanced Raman scattering (SERS) substrates for unlabelled molecular sensing. The addition of CTAB enables not only the electromagnetic enhancement by controllable producing Ag NAs “hotspots”, but also the signal enhancement by enriching probe molecules via hydrophobic interaction. Two concentration regimes of 1.0 × 10−8–1.0 × 10−11 M and 1.0 × 10−12–1.0 × 10−16 M have been obtained for quantitative and qualitative detection of Rhodamine 6G (R6G) in aqueous solution, respectively. As a result, for determination of R6G, the quantitative and qualitative detection limits of 1.0 × 10−11 and 1.0 × 10−16 M have been obtained, respectively, with high reproducibility showing the relative standard deviation (RSD) of ∼7.3%. Simulation has been carried out using finite-difference time-domain (FDTD) to evaluate the dependence of electric field on the size and inter-gap of Ag NPs, showing good agreement with experimental results. The high sensitivity also enables SERS characterization of non-resonant and low Raman cross-section biomolecules, for example, amino acids. Such a fabrication process is simple, fast, cheap and reproducible; and therefore, it would be helpful to produce high sensitive SERS substrates to broaden their applications in chemical and biological fields for molecular diagnostics to single-/multiple-molecule detection.

One-pot synthesis of poly (acrylic acid)-stabilized Fe3O4 nanocrystal clusters for the simultaneously qualitative and quantitative detection of biomarkers in lateral flow immunoassay

Lateral flow immunoassay (LFIAs) has found widespread applications in point-of-care testing (POCT). However, conventional LFIAs based on gold nanoparticles can only provide limited information (qualitative or semi-quantitative information) and suffer from low sensitivity. To address this issue, we developed a Fe3O4 nanocrystal cluster-based highly sensitive LFIAs for the simultaneously qualitative and quantitative detection of trace-level biomarkers. The synthesis of poly (acrylic acid)-stabilized superparamagnetic nanocrystal clusters (PAA-MNCs) is a one-pot, simple and convenient technique, and the polyelectrolyte coating provides enough stability, good dispersity and downstream conjugation sites. Using these PAA-MNCs as a label nanomaterial in LFIAs, a model biomarker (amino-terminal pro-B-type natriuretic peptide (NT-proBNP) antibody) was detected qualitatively and quantitatively. The results show that tests have a qualitative detection limit of 100 pg/mL and a quantitative linear relationship between the magnetic signal and antibody concentration (20–8000 pg/mL) under the optimized experimental conditions. The developed LFIA based on PAA-MNCs for NT-proBNP could be used for the clinical assessment of heart failure, offering tremendous potential for personalized medicine.

Modeling of Chromium, Copper, Zinc, Arsenic and Lead Using Portable X-ray Fluorescence Spectrometer Based on Discrete Wavelet Transform.

A modeling method based on discrete wavelet transform (DWT) was introduced to analyze the concentration of chromium, copper, zinc, arsenic and lead in soil with a portable X-ray fluorescence (XRF) spectrometer. A total of 111 soil samples were collected and observed. Denoising and baseline correction were performed on each spectrum before modeling. The optimum conditions for pre-processing were denoising with Coiflet 3 on the 3rd level and baseline correction with Coiflet 3 on the 9th level. Calibration curves were established for the five heavy metals (HMs). The detection limits were compared before and after the application of DWT, the qualitative detection limits and the quantitative detection limits were calculated to be three and ten times as high as the standard deviation with silicon dioxide (blank), respectively. The results showed that the detection limits of the instrument using DWT were lower, and that they were below national soil standards; the determination coefficients (R2) based on DWT-processed spectra were higher, and ranged from 0.990 to 0.996, indicating a high degree of linearity between the contents of the HMs in soil and the XRF spectral characteristic peak intensity with the instrument measurement.

Rapid lateral-flow immunoassay for the quantum dot-based detection of puerarin

In this study, a rapid (within 10min) quantitative lateral-flow immunoassay using a quantum dots (QDs)-antibody probe was developed for the analysis of puerarin (PUE) in water and biological samples. The competitive immunoassay was based on anti-PUE monoclonal antibody conjugated with QDs (detection reagent). Secondary antibody was immobilized on one end of a nitrocellulose membrane (control line) and PUE-bovine serum albumin conjugate was immobilized on the other end (test line). In the quantitative experiment, the detection results were scanned using a membrane strip reader and a detection curve (regression equation: y=−0.11ln(x)+0.979, R2=0.9816) representing the averages of the scanned data was obtained. This curve was linear from 1 to 10μg/mL. The IC50 value was 75.58ng/mL and the qualitative detection limit of PUE was 5.8ng/mL. The recovery of PUE added to phosphate-buffered saline and biological samples was in the range of 97.38–116.56%. To our knowledge, this is the first report of the quantitative detection of a natural product by QDs-based immunochromatography, which represents a powerful tool for rapidly screening PUE in plant materials and other biological samples.

Installation and measurement capacity of 3 × 592 GBq 241Am–Be neutron irradiation cell

Abstract In this study, the installation and measurement capacity of the neutron irradiation system are investigated. First of all an irradiation geometry enabling optimum irradiation was designed for three 241Am–Be sources each of it having 592 GBq activity. Neutron irradiation system was installed after design and optimization of the system including the design of appropriate moderator and shielding were completed. Radiation safety standards of the Neutron Research Laboratory fulfilling the requirements of national regulation were achieved with unique configuration of the shielding materials. In this study the results of qualitative and quantitative detection limits obtained for Na, Al, Cl, K, Ti, V, Mn, Fe, Co, Cu, Zn, Ga, Ge, As, Se, Br, Rb, Sr, Y, Mo, Ru, Ag, Cd, In, Sb, I, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Yb, Lu, Hf, W, Pt, Au, Th and U elements by using the neutron irradiation cell comprising 3 × 592 GBq 241Am–Be isotopic neutron source are presented and discussed.

Quantitative Determination of Proteins Based on Strong Fluorescence Enhancement in Curcumin-Chitosan-Proteins System

We found that the fluorescence intensity of curcumin (CU) can be highly enhanced by protein bovine serum albumin (BSA) and human serum albumin (HSA) in the presence of chitosan (CTS). Based on this finding, a new fluorimetric method to determine the concentration of protein was developed. Under optimized conditions, the enhanced intensities of fluorescence are quantitatively in proportion to the concentrations of protein in range of 0.007-100 μg·mL(-1) for BSA and 0.004-100 μg·mL(-1) for HSA at 426 nm excitation, and 0.007-100 μg·mL(-1) for BSA and 0.01-100 μg·mL(-1)for HSA at 280 nm excitation, while corresponding qualitative detection limits (S/N = 3) can lower to 3.96, 2.46, 4.56, 9.20 ng·mL(-1), respectively. The method has been successfully used for the determination of HSA in real samples. Based on resonance light scattering and UV-visible absorption spectroscopic analysis, mechanism studies suggested that the highly enhanced fluorescence of CU was resulted from synergic effects of favorable hydrophobic microenvironment provided by BSA and CTS and efficient intermolecular energy transfer between BSA and CU. Protein BSA may bind to CTS through hydrogen bonds, which causes the protein conformation to convert from β-fold to α-helix. CU can combine with the BSA-CTS complex through its center carbonyl carbon, and CTS plays a key role in promoting the energy transfer process by shortening the distance between BSA and CU.

Assessment of Aspergillus fumigatus in Guinea Pig Bronchoalveolar Lavages and Pulmonary Tissue by Culture and Realtime Polymerase Chain Reaction Studies

In this study we pursued a diagnostic target in Aspergillus fumigatus (AF) by using qualitative Realtime PCR combined with proprietary DNA primers and a hydrolysis probe specific for this fungal target. Qualitative Realtime PCR is a diagnostic tool that utilizes Realtime PCR technology and detects the presence or absence target specific DNA within a predetermined detection range. Respiratory tissue and fluids from experimentally infected guinea pigs were tested by extracting DNA from the samples which were amplified and detected using AF specific DNA primers and probe. This study included qualitative evaluations of all specimens for the presence of the DNA of AF. The findings in the tissues after AF infection were compared to the numbers of spores in aerosolized samples used to inoculate the animals. Results demonstrated that the specific probe and primer set could detect the presence or absence of AF DNA in the sample. The qualitative detection limit of the assay ranged from 6 × 104 copies to 6 copies. Since blood cultures are rarely positive for Aspergillosis, our data indicate that qualitative Realtime PCR, in combination with the appropriate DNA primers and probe can serve as an effective diagnostic tool in the early detection of fungal infections.

Event-specific qualitative and quantitative detection of transgenic rice Kefeng-8 by characterization of the transgene flanking sequence

The transgenic rice line Kefeng-8 harboring insect-resistant genes Cry1Ac and CpTI showed ideal field performances characterized by high resistance to rice stem borer (Scirpophaga incertulas) and leaf roller (Cnaphalocrocis medinalis). This GM rice line is likely to be approved in China in the near future. In this study, we estimated the insert number of foreign genes, analyzed the flanking sequences of T-DNA in rice genome, and presented an event-specific detection method for this line. The results show that the foreign gene inserted one copy between position 11,774 and 11,805 of chromosome 11 (AC120536.5) in Kefeng-8 genome. Based on these inserts and border sequences, the event-specific qualitative and quantitative PCR system was established for Kefeng-8. The qualitative detection limit was assessed to be 0.1%, and the limit of quantitative method was assessed to be 100 initial template copies. Two mixed rice sample with known Kengfeng-8 contents were used to verify the quantitative method, from which the expected results were observed. This study provides a reliable method and information for detection, identification, and quantification of the presence of GM rice Kefeng-8.

A screening lateral flow immunochromatographic assay for on-site detection of okadaic acid in shellfish products

A lateral flow immunochromatographic (LFIC) test strip based on a colloidal gold–monoclonal antibody (McAb) conjugate was developed for on-site rapid detection of okadaic acid (OA) in shellfish. It applies a competitive format using an immobilized toxin conjugate and free toxin present in samples. The McAb against OA was conjugated with 20-nm colloidal gold as detector reagent. The toxin in the sample competed with the immobilized toxin to bind to the gold conjugated with McAb. The colloidal gold/McAb/toxin mobile complex was not captured by OA–bovine serum albumin (BSA) on the test line, but it was captured by goat anti-mouse immunoglobulin G (IgG) on the control line. The color density of the test line correlated with the concentration of toxin in the range of 10–50ngml−1. The qualitative detection limit of 150μgkg−1 sample was close to the European Union (EU) regulatory limit (160μgkg−1). Therefore, these strips were able to directly and qualitatively estimate the consuming safety of shellfish. They require no equipment because of available visual results, and they screened numerous samples within 10min. The results were further confirmed by high-performance liquid chromatography tandem mass spectrometry (HPLC–MS/MS). As a food safety screening tool, the test strips are convenient and useful to rapidly on-site test the presence of OA in shellfish products.

Sensitive Detection of Shiga Toxin 2 and Some of Its Variants in Environmental Samples by a Novel Immuno-PCR Assay

Shiga toxin-producing Escherichia coli (STEC) in the environment has been reported frequently. However, robust detection of STEC in environmental samples remains difficult because the numbers of bacteria in samples are often below the detection threshold of the method. We developed a novel and sensitive immuno-PCR (IPCR) assay for the detection of Shiga toxin 2 (Stx2) and Stx2 variants. The assay involves immunocapture of Stx2 at the B subunit and real-time PCR amplification of a DNA marker linked to a detection antibody recognizing the Stx2 A subunit. The qualitative detection limit of the assay is 0.1 pg/ml in phosphate-buffered saline (PBS), with a quantification range of 10 to 100,000 pg/ml. The IPCR method was 10,000-fold more sensitive than an analogue conventional enzyme-linked immunosorbent assay (ELISA) in PBS. Although the sensitivity of the IPCR for detection of Stx2 was affected by environmental sample matrices of feces, feral swine colons, soil, and water from watersheds, application of the IPCR assay to 23 enriched cultures of fecal, feral swine colon, soil, and watershed samples collected from the environment revealed that the IPCR detected Stx2 in all 15 samples that were shown to be STEC positive by real-time PCR and culture methods, demonstrating a 100% sensitivity and specificity. The modification of the sandwich IPCR we have described in this study will be a sensitive and specific screening method for evaluating the occurrence of STEC in the environment.

Modification of mid-point restrictor of heart cut multidimensionalgas chromatography-mass spectrometry system and its application in analysis of benzo［<I>a</I>］pyrene in cigarette smoke

The mid-point restrictor, known as the key spare part of multidimensional gas chromatography (MDGC), was modified and applied in the determination of benzo[a] pyrene in cigarette smoke. The graphite restrictor was replaced by a 0.25 mm i.d. fused silica open tubular and the two-hole graphite ferrule was replaced by a press-fit glass Y-splitter to improve the stability of retention time on the 1st dimensional column and eliminate the carry-over effects of graphite. The cigarette samples were prepared as follows: The mainstream cigarette smoke collected on Cambridge pad was extracted with cyclohexane, then the extractant was analyzed by heart cut MDGC-mass spectrometry (MS) directly with benzo [ a] pyrene-d12 as internal standard. The method was proved to be simple, sensitive, fast and reliable with good linearity (linear range of 1.47-29.4 microg/L, r2 of 0.9999), reproducibility (relative standard deviation (RSD) of 1.94%), recovery (90.74%-101.86%) and low quantitative and qualitative detection limits. Moreover, the amount of benzo [a] pyrene in the 2R4F Kentucky reference cigarette smoke obtained by this method was close to that reported in literature.

Determination of Protein by Fluorescence Enhancement of Curcumin in Lanthanum-Curcumin-Sodium Dodecyl Benzene Sulfonate-Protein System

We found that the fluorescence intensity of the lanthanum (La(3+))-curcumin (CU) complex can be highly enhanced by proteins in the presence of sodium dodecyl benzene sulphonate (SDBS). Based on this finding, a new fluorimetric method for the determination of protein was developed. Under optimized conditions, the enhanced intensities of fluorescence are quantitatively in proportion to the concentrations of proteins in the range 0.0080-20.0 μg·mL(-1) for bovine serum albumin (BSA) and 0.00080-20.0 μg·mL(-1) for human serum albumin (HSA) with excitation of 425 nm, and 0.00020-20.0 μg·mL(-1) for bovine serum albumin (BSA) and 0.00080-20.0 μg·mL(-1)for human serum albumin (HSA) with excitation of 280 nm, while corresponding qualitative detection limits (S/N ≥ 3) are as low as 5.368, 0.573, 0.049, 0.562 µg·mL(-1), respectively. Study on reaction mechanism reveals that proteins can bind with La(3+), CU and SDBS through self-assembling function with electrostatic attraction, hydrogen bonding, hydrophobic interaction and van der Waals forces, etc. The proteins form a supermolecular association with multilayer structure, in which La(3+)-CU is clamped between BSA and SDBS. The unique high fluorescence enhancement of CU is resulted through synergic effects of favorable hydrophobic microenvironment provided by BSA and SDBS, and efficient intermolecular energy transfer among BSA, SDBS and CU. In energy transfer process, La(3+) plays a crucial role because it not only shortens the distance between SDBS and CU, but also acts as a "bridge" for transferring the energy from BSA to CU.

Development of an immunochromatographic assay for the rapid detection of chlorpyrifos-methyl in water samples

A rapid (less than 10 min), qualitative and semi-quantitative immunochromatography using colloidal gold-antibody probe was successfully developed and applied in determination of chlorpyrifos-methyl (a wide-spectrum organophosphorus pesticide) in water samples. The qualitative detection limit of chlorpyrifos-methyl was determined as 0.6 μg ml −1 by using immunochromatography. In the semi-quantitative experiment, the detection results of chlorpyrifos-methyl were scanned by a membrane strip reader, and a detection curve representing the scanned data average was obtained. After conversion, it was observed that in the range of 50 – 12,150 ng ml −1, the graph between logit( B/ B 0) and logarithm of concentration of chlorpyrifos-methyl was linear, from which, the regression equation ( y = −2.5229 x + 7.5951, R 2 = 0.9889) and IC 50 value (1024.39 ng ml −1) was obtained, respectively. Meanwhile, the detection limit was calculated as 132.91 ng ml −1 by the extrapolation of B 0 − 2SD. In addition, the cross-reactivities were less than 1% with tested analog compounds and regarded as negligible. The recoveries obtained by standard chlorpyrifos-methyl addition to water samples were 102.5–107.6%. Overall, to our knowledge, this is the first report of qualitative and semi-quantitative detection of chlorpyrifos-methyl by immunochromatography.

Plasmon Enhancement and Surface Wave Quenching for Phase Ratiometry in Coextraction-Based Fluorosensors

In this study, a novel fluorescence ratiometric sensing scheme is presented. Gold nanoparticles (GNPs) were lipophilized with dodecanethiol and incorporated in the ether phase of a coextraction based ammonium sensor. The novel concept of this sensing scheme is that the analyte response involves a movement of the fluorophore toward lipophilized GNPs in an organic phase. Properly arranged, the system benefits from surface plasmon enhancement as well as increased lossy surface wave quenching as the fluorophore moves toward the GNPs. Likely constructive scattering effects are also present due to some build-up of nanoparticle clusters. The sensor configuration significantly reduced the noise level, increased the ratiometric signal, and improved the limit of detection approximately 3 orders of magnitude as compared with the optical sensor without the nanoparticles and ion-selective ammonium electrodes. Qualitative and quantitative detection limits were 1.7 and 5.7 nM, respectively. The sensing scheme is versatile and can be utilized for many other ions.

Visible Raman spectroscopy for the discrimination of olive oils from different vegetable oils and the detection of adulteration

AbstractWe have investigated the potential of Raman spectroscopy with excitation in the visible spectral range (VIS Raman) as a tool for the classification of different vegetable oils and the quantification of adulteration of virgin olive oil as an example. For the classification, principal component analysis (PCA) was applied, where 96% of the spectral variation was characterized by the first two components. A significant similarity between sunflower oil and extra‐virgin olive oil was found using this approach. Therefore, sunflower oil is a potential candidate for adulteration in most commercially available olive oils. Beside the classification of the different vegetable oils, we have successfully applied Raman spectroscopy in combination with partial least‐squares (PLS) regression analysis for very fast monitoring of adulteration of extra‐virgin olive oil with sunflower oil. Different mixtures of extra‐virgin olive oil with three different sunflower oil types were prepared between 5 and 100% (v/v) in 5% increments of sunflower oil. While in the present context the adulteration usually refers to the addition of reasonable amounts of the adulterant (given the similarity with the basic product), we show that the technique proposed can also be used for trace analysis of the adulterant. Without using techniques like surface‐enhanced Raman scattering (SERS), a quantitative detection limit down to 500 ppm (0.05%) could be achieved, a limit irrelevant for adulteration in commercial terms but significant for trace analysis. The qualitative detection limit even was at considerably lower concentration values. Based on PCA, a clear discrimination between pure extra‐virgin olive oil and olive oil adulterated with sunflower oil was achieved. The adulterant content was successfully determined using PLS regression with a high correlation coefficient and small root mean‐square error for both prediction and validation. Copyright © 2009 John Wiley & Sons, Ltd.